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Diethyl (aminomethyl)phosphonate → HCID 20229893, 화합물

HRID 2290680
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HRID 2290680 반응식
[NH2:1][CH2:2][P:3](=[O:10])([O:7][CH2:8][CH3:9])[O:4][CH2:5][CH3:6].[F:11][C:12]([F:33])([F:32])[C:13]1[CH:14]=[CH:15][C:16]([O:19][C:20]2[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[C:22]([N+]([O-])=O)[CH:21]=2)=[N:17][CH:18]=1>C1(C)C=CC=CC=1>[N+:26]([C:23]1[CH:22]=[CH:21][C:20]([O:19][C:16]2[CH:15]=[CH:14][C:13]([C:12]([F:33])([F:11])[F:32])=[CH:18][N:17]=2)=[CH:25][C:24]=1[NH:1][CH2:2][P:3](=[O:10])([O:7][CH2:8][CH3:9])[O:4][CH2:5][CH3:6])([O-:28])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1596920Diethyl (aminomethyl)phosphonateHCID 202299032-(3,4-Dinitrophenoxy)-5-(trifluoromethyl)pyridine

생성물 1

HCID 20229893HCID 20229893, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

With stirring, 7.6 g (0.045 mole) of diethyl aminomethylphosphonate are added dropwise to a solution of 15 g (0.045 mole) of (5-trifluoromethyl-2-pyridyloxy)-3,4-dinitrobenzene in 50 ml of toluene, and the mixture is heated for 12 hours to reflux. The mixture is then concentrated and the residue is chromatographed over silica gel with a 1:4 mixture of hexane/ethyl acetate, affording 9.8 g (48.7% of theory) of the title compound with a melting point of 74°-76° C.

후처리

  1. temperaturethe mixture is heated for 12 hours
  2. temperatureto reflux
  3. concentrationThe mixture is then concentrated
  4. customthe residue is chromatographed over silica gel with a 1:4 mixture of hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-f12330553e9349cc852dc3c5d242daf7
출처 데이터셋
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04618358

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